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Microwave digestion pretreatment method for soil detection-total sodium potassium calcium content determination

A microwave digestion and soil detection technology, applied in the field of environmental detection, can solve the problems of time-consuming, labor-intensive and acid-consuming digestion, easy to cause large errors, easy to introduce other impurities, etc., to achieve complete digestion, less sample pollution, and optimized digestion process. Effect

Inactive Publication Date: 2016-11-09
SHANGHAI INST OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] For example, some current national standards in my country have the following methods for measuring soil total sodium, potassium and calcium. The digestion is time-consuming, labor-intensive and acid-consuming, and the procedures are complicated and cumbersome, which may easily cause large errors or introduce other impurities:

Method used

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Examples

Experimental program
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Effect test

Embodiment 1

[0032] (1) Take the pretreated and sieved soil sample with a particle size less than 0.5mm, put it in a 50mL polytetrafluoroethylene digestion tube, the weight is 0.2500g, and the accuracy is 0.0001g, add 9mL concentrated Nitric acid, 3mL hydrofluoric acid and 2mL hydrogen peroxide, when adding the above acid, wash the soil on the wall of the digestion tube with acid to the bottom of the tube, and then carry out microwave digestion. The concentrated nitric acid, hydrofluoric acid, hydrogen peroxide used and perchloric acid are superior grade pure;

[0033] (2) The steps of microwave digestion are as follows: 1000w ramp time 2 minutes to 100°C; 1000w ramp time 1.5 minutes to 150°C; 1000w ramp time 1.5 minutes to 185°C, keep for 15 minutes;

[0034] (3) Cool down after microwave digestion, the digestion solution does not need to be transferred to other vessels, just continue to wash out the acid in the digestion tube, use the acid washer to wash the sample solution in the digest...

Embodiment 2

[0037] (1) Take the pretreated and sieved soil sample with a particle size of less than 0.5mm, put it in a 50mL polytetrafluoroethylene digestion tube, the weight is 0.3000g, and the accuracy is 0.0001g, add 9mL concentrated Nitric acid, 3mL hydrofluoric acid and 2mL hydrogen peroxide, when adding the above acid, wash the soil on the wall of the digestion tube with acid to the bottom of the tube, and then carry out microwave digestion. The concentrated nitric acid, hydrofluoric acid, hydrogen peroxide used and perchloric acid are superior grade pure;

[0038] (2) The steps of microwave digestion are as follows: 1000w ramp time 2 minutes to 100°C; 1000w ramp time 1.5 minutes to 150°C; 1000w ramp time 1.5 minutes to 185°C, keep for 15 minutes;

[0039] (3) Cool down after microwave digestion, the digestion solution does not need to be transferred to other vessels, just continue to wash out the acid in the digestion tube, use the acid washer to wash the sample solution in the dig...

Embodiment 3

[0042] (1) Take the pretreated and sieved soil sample with a particle size less than 0.5mm, put it in a 50mL polytetrafluoroethylene digestion tube, the weight is 0.4000g, and the accuracy is 0.0001g, add 9mL concentrated Nitric acid, 3mL hydrofluoric acid and 2mL hydrogen peroxide, when adding the above acid, wash the soil on the wall of the digestion tube with acid to the bottom of the tube, and then carry out microwave digestion. The concentrated nitric acid, hydrofluoric acid, hydrogen peroxide used and perchloric acid are superior grade pure;

[0043] (2) The steps of microwave digestion are as follows: 1000w ramp time 2 minutes to 100°C; 1000w ramp time 1.5 minutes to 150°C; 1000w ramp time 1.5 minutes to 185°C, keep for 15 minutes;

[0044] (3) Cool down after microwave digestion, the digestion solution does not need to be transferred to other vessels, just continue to wash out the acid in the digestion tube, use the acid washer to wash the sample solution in the digest...

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Abstract

The invention discloses a microwave digestion pretreatment method for soil detection-total sodium potassium calcium content determination. The microwave digestion pretreatment method is used for determining the total sodium content, the total potassium content and the total calcium content in soil, a pretreated soil sample is placed into a polytetrafluoroethylene digestion tube, concentrated nitric acid, hydrofluoric acid and hydrogen peroxide are added into the digestion tube, and then microwave digestion is carried out; cooling is carried out after digestion, and an acid catching instrument is used for carrying out acid catching on a sample solution contained in the digestion tube; after acid catching is completed, nitric acid of 1-3% (v / v) is used for dissolving residues in the digestion tube and volume setting to obtain solution after soil pretreatment, and the total potassium content and the total calcium content of the solution are determined. The step of acid catching is added, measurement results are more accurate, damage to the experiment instrument due to overhigh acidity is avoided, the soil is digested more thoroughly, element content determination is higher in accuracy, and in addition compared with existing method of determining the total sodium potassium calcium content in the soil, the method is simpler and easier to implement.

Description

technical field [0001] The invention relates to the field of environmental detection, in particular to a soil detection-a microwave digestion pretreatment method for measuring the content of total sodium, potassium and calcium. Background technique [0002] In the scientific research industry of soil research, especially in the improvement and restoration of saline-alkali land, it is often involved in the determination of the total sodium, total potassium and total calcium content of the soil. The key step in determining soil total sodium, total potassium, and total calcium is the soil pretreatment method, which is different from the pretreatment method for determining soil heavy metals, and the soil pretreatment method for determining soil total sodium, total potassium, and total calcium. It is more prone to incomplete digestion, large measurement errors and the introduction of impurities, and the operation process is cumbersome and complicated. At present, the soil pretre...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N1/44
CPCG01N1/44
Inventor 杜三艳陈小华方龙伟杜乃强高欢潘栋宇
Owner SHANGHAI INST OF TECH
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